US5922099A - Apparatus and method for fabricating tube-shaped glass monolith using sol-gel process - Google Patents

Apparatus and method for fabricating tube-shaped glass monolith using sol-gel process Download PDF

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Publication number
US5922099A
US5922099A US09/037,525 US3752598A US5922099A US 5922099 A US5922099 A US 5922099A US 3752598 A US3752598 A US 3752598A US 5922099 A US5922099 A US 5922099A
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United States
Prior art keywords
gel
mold
tube
sol
set forth
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Expired - Fee Related
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US09/037,525
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English (en)
Inventor
Young-Sik Yoon
Young-Min Baik
Sun-Uk Kim
Myung-Chul Jun
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Samsung Electronics Co Ltd
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Samsung Electronics Co Ltd
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Priority claimed from KR1019970007976A external-priority patent/KR100241969B1/ko
Priority claimed from KR1019970007972A external-priority patent/KR100229899B1/ko
Application filed by Samsung Electronics Co Ltd filed Critical Samsung Electronics Co Ltd
Assigned to SAMSUNG ELECTRONICS CO., LTD. reassignment SAMSUNG ELECTRONICS CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BAIK, YOUNG-MIN, JUN, MYUNG-CHUL, KIM, SUN-UK, YOON, YOUNG-SIK
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
    • C03B37/01—Manufacture of glass fibres or filaments
    • C03B37/012—Manufacture of preforms for drawing fibres or filaments
    • C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
    • C03B37/016—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by a liquid phase reaction process, e.g. through a gel phase
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/12—Other methods of shaping glass by liquid-phase reaction processes
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
    • C03C1/006—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S65/00—Glass manufacturing
    • Y10S65/09—Tube
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S65/00—Glass manufacturing
    • Y10S65/90—Drying, dehydration, minimizing oh groups
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S65/00—Glass manufacturing
    • Y10S65/901—Liquid phase reaction process

Definitions

  • the present invention relates to an optical fiber forming glass tube fabricating method using a sol-gel process, and in particular, to an apparatus and method for fabricating a tube-shaped glass monolith using a sol-gel process, which can direct a moist gel to unidirectionally dry and shrink.
  • an optical fiber preform is fabricated by inside deposition such as MCVD (Modified Chemical Vapor Deposition) or outside deposition such as VAD (Vapor phase Axial Deposition) and OVD (Outside Vapor Deposition).
  • MCVD is most generally used in fabrication of high-quality optical fibers.
  • a preform is fabricated using a high-purity glass tube by inside deposition and overcladding.
  • the glass tube essentially used in the MCVD is more pure and more cost-competitive when fabricated using a sol-gel process than that fabricated by other technology.
  • a glass tube is fabricated in a general sol-gel process as follows.
  • a first sol is formed by dispersing fine fumed silica particles in deionized water to prevent cracking.
  • the first sol is than gelled and the gel is then dried.
  • the dried first gel becomes powder through grinding and classification, is thermally treated, and is re-dispersed in deionized water.
  • a second sol is formed.
  • the second sol is gelled in a mold, removed from the mold, dried, and then sintered to form a glass monolith.
  • the powder is redispersed in water, having its pH adjusted by the addition of an acid, to form a second sol, cast in molds of glass tubing and rubber stoppers to gel.
  • the gel is removed from the mold, dried and sintered to form a low alkali silica glass.
  • Other molds are discussed in U.S. Pat. No. 4,419,115 to David W. Johnson, Jr., et al., entitled Fabrication Of Sintered Hih-Silica Glasses, U.S. Pat. No. 4,786,302 to Haruo Osafune, et al., entitled, Method Of Preparing Tubular Silica Glass and U.S. Pat. No. 5,352,259 to Masato Oku, et al., entitled Method Of Manufacturing Optical Fiber Preform.
  • Some conventional gel drying method is limited in molding a dried gel to a thickness of 15 mm or above due to the difference between shrinkage rates of the inner and outer surfaces of the tube-shaped gel when it is dried. It is very difficult to mold the gel into a tube shape because the outer and inner surfaces of the moist gel are concurrently dried and thus develop shrinkage stresses. In addition, the moist gel is dried for a long time at constant temperature and humidity, thereby increasing fabrication cost and making it impossible to extend the gel lengthwise.
  • the dried gel is vulnerable to cracking even at a slight impact, and should be at least about 1 m long to mold an optical fiber forming glass tube.
  • a conventional tube-shaped glass forming mold cannot relieve the gel of stresses caused by uniformless shrinkage in a lower portion of the gel due to longitudinal load of the moist gel.
  • the dried gel is highly vulnerable to cracking, cannot be further extended lengthwise, and is unsuitable for an optical fiber forming glass tube.
  • An object of the present invention is to provide a tube-shaped glass monolith fabricating apparatus using a sol-gel process, which can fabricate a large crack-free glass tube for use in fabricating an optical fiber by minimizing stresses on a gel caused by the shrinkage of the gel during drying a moist gel.
  • Another object of the present invention is to provide a tube-shaped glass monolith fabricating apparatus using a sol-gel process, which can extend a gel lengthwise by distributing and reducing a shrinking force imposed on a lower portion of a moist gel and the load of the gel.
  • Still another object of the present invention is to provide a tube-shaped glass monolith fabricating method using a sol-gel process, which can fabricate a large glass tube by unidirectionally drying a tube-shaped moist gel.
  • Still yet another object of the present invention of the present invention is to provide a tube-shaped glass monolith fabricating method using a sol-gel process, which can prevent a gel from cracking during drying the gel by directing the gel to shrink from outside to inside.
  • a further object of the present invention is to provide a tube-shaped glass monolith fabricating method using a sol-gel process, which can fabricate an optical fiber forming overcladding tube.
  • a tube-shaped glass monolith fabricating apparatus using a sol-gel process has an upper mold having cylindrical portions of different sizes and a first fixing hole in the center thereof.
  • a lower mold has a second fixing hole in the center thereof, a first lower cylindrical portion inclined toward the center thereof to minimize stresses generated during the gelation or drying step, and a second lower cylindrical portion having a vacuum releasing hole to prevent vacuum-induced stresses during the drying step.
  • a central mold is disposed between the upper mold and the lower mold, a sol is poured therein gelation and drying steps are performed on the sol.
  • a rod-shaped rod is installed along the central longitudinal axis of the central mold, for molding a gel into a tube after the drying step.
  • a tube-shaped glass monolith fabricating method using a sol-gel process there is provided a tube-shaped glass monolith fabricating method using a sol-gel process.
  • a tube-shaped glass monolith fabricating apparatus which has an upper mold including cylindrical portions of different sizes, a lower mold including a first lower cylindrical portion inclined toward the center thereofby a predetermined degree and a second lower cylindrical portion having a vacuum releasing hole, a cylindrical central mold for forming a tube-shaped glass, and a rod-shaped rod, the lower mold, the central mold, and the rod are assembled and a sol is poured in the central mold. Then, an unmixable liquid is poured on the sol, and the upper mold is assembled to the central mold.
  • the sol is gelled in the central mold, the upper mold is removed, a cap is opened to release vacuum, and the rod is removed. A small amount of the unmixable liquid remains in a gel hole formed in the center of the gel and the vacuum releasing hole is filled with the cap. An upper portion of the gel hole is sealed with a sealing paper. Subsequently, the gel is dried for a predetermined time, the central mold is removed from the gel, and the gel is dried until the gel completely shrinks. Finally, the sealing paper and the unmixable liquid are removed from the gel. Thus, a tube-shaped dried gel is formed.
  • FIG. 1 is an exploded perspective view of a mold for forming a tube-shaped glass monolith in a sol-gel process according to a preferred embodiment of the present invention
  • FIG. 2 is a side sectional view of the assembled mold for fabricating a tube-shaped glass monolith in a sol-gel process, referred to for depicting a gelation step of a tube-shaped glass monolith fabricating method using a sol-gel process, according to the preferred embodiment of the present invention
  • FIG. 3 is a side sectional view of the mold, for depicting a drying step of the tube-shaped glass monolith fabricating method using a sol-gel process according to the preferred embodiment
  • FIG. 4 is a plan view of the mold shown in FIG. 3.
  • FIG. 1 is an exploded perspective view of a mold for forming a tube-shaped glass monolith in a sol-gel process according to a preferred embodiment of the present invention
  • FIG. 2 is a side sectional view of the assembled mold for fabrication of a tube-shaped glass monolith in a sol-gel process according to the preferred embodiment of the present invention.
  • a mold for use as a tube-shaped glass monolith fabricating apparatus using a sol-gel process is divided into an upper mold 10 (a stepped upper lid), a lower mold 26 (a stepped lower lid), a central mold 18, and a rod 24.
  • Elements 10, 18, 24, and 26 each have smooth surfaces which contact the sol and are formed of polystyrene, polypropylene, teflon, or steel in order to mold a thick-wall tube.
  • the upper mold 10 is comprised of a first upper cylindrical portion 12 to be mounted on the central mold 18 and a second upper cylindrical portion 16 having a diameter smaller that the diameter of the first upper cylindrical portion 12 to engage with the inner surface of central mold 18. That is, the first and second upper cylindrical portions 12 and 16 are integrally formed and have a first fixing hole 14 in the centers thereof, for inserting the rod 24.
  • the central mold 18 is cylindrical and has a bore 22 for retaining the fumed silica in the sol state during sol formation, gelation, and drying steps.
  • the upper surface of the central mold 18 is a first mounting surface 20 for mounting the first upper cylindrical portion 12 of the upper mold 10 thereon.
  • the rod 24 is to enable a gel to be formed into a tube and the central axis of rod 24 is coincident with the central axis of central mold 18.
  • the lower mold 26 is comprised of a first lower cylindrical portion 28 to be inserted into the bore 22 of the central mold 18, and a second lower cylindrical portion 32 for mounting the central mold 18 thereon. That is, the first and second lower cylindrical portions 28 and 32 are integrally formed and have a second fixing hole 30 in the centers thereof, for inserting the rod 24.
  • the upper surface of the first lower cylindrical portion 28 is an inclined surface 28a inclined toward the center of the lower mold 26 by about 5-45° to minimize the downward shrinkage force of a gel and pressure generated from the inside of the gel to the outside thereof during a gelation or drying step.
  • the inclined surface 28a may be conical within about 5-45°.
  • a vacuum releasing hole 34 is formed into one side surface of the second lower cylindrical portion 32, communicating with the second fixing hole 30, so that vacuum-induced stresses are not generated inside a tube-shaped gel when the rod 24 is removed to dry a moist gel molded from a sol.
  • the vacuum releasing hole 34 is generally closed by a cap 36, as shown in FIG. 2.
  • a sol is formed by mixing fumed silica with deionized water. Then, as shown in FIG. 2, the vacuum releasing hole 34 of the second lower cylindrical portion 32 is plugged with the cap 36, and the rod 24 is fixedly inserted into the second fixing hole 30 in the center of the lower mold 26. Then, the central mold 18 is mounted on the second mounting surface 32a of the second lower cylindrical portion 32, and the sol is poured in the bore 22 of the central mold 18 to a predetermined height. An unmixable liquid 102 unmixable with water and having a lower specific gravity than water is poured on the upper surface of the sol to prevent the sol from contacting outside air.
  • the unmixable liquid 102 is kerosine.
  • the second upper cylindrical portion 16 of the upper mold 10 is fixedly inserted into the bore 22.
  • the first upper cylindrical portion 12 is mounted on the first mounting surface 20 of the central mold 18 and, simultaneously, the rod 24 is fixedly inserted into the first fixing hole 14 in the center of the upper mold 10.
  • the sol is gelled in the central mold 18 for about 24-72 hours.
  • about 1% or less of an organic polymer is added to the sol, or the pH of the sol may be controlled.
  • the upper mold 10 is removed, the vacuum releasing hole 34 in the second lower cylindrical portion 32 is opened by removing the cap 36, and the rod 24 is slowly retracted upward. At this time, air is introduced into the vacuum releasing hole 34 and the second fixing hole 30, that is, no vacuum occurs during the removal of rod 24.
  • the unmixable liquid 102 flows into the gel hole 106 and comes out through the vacuum releasing hole 34, as shown in FIG. 3. Then, the unmixable liquid 102 is continuously evacuated by a predetermined amount, and the vacuum releasing hole 34 is again plugged with the cap 36 when the unmixable liquid 102 remaining in the gel hole 106 (see FIG. 3) is at a height of 10 mm, in order to prevent outside air from contacting a lower portion of the gel 100.
  • an upper portion of the gel hole 106 is sealed with a sealing paper 104 to prevent shrinkage inside the gel hole 106, to regulate only the outside shrinkage of the gel hole 106, and to prevent the gel 100 from cracking.
  • the sealing paper 104 is formed of wax paper, wrap film, or vinyl to be large enough to cover the gel hole 106.
  • the central mold 18 is removed from the lower mold 26 and the moist gel 100 dried for about 3-7 days until the moist gel 100 is strong enough to resist cracking. Then, the sealing paper 104 is removed from the upper portion of the gel 100, and the remaining unmixable liquid 102 is removed from the gel hole 106 by opening the vacuum releasing hole 34. Then, the lower mold 26 is removed from the gel 100, thereby obtaining a crack-free dried tube-shaped gel 100.
  • the dried gel 100 is thermally treated at about 600-900° C. to be used for fabricating an optical fiber, and sintered at about 1300-1450° C.
  • an optical fiber forming overcladding tube is completed.
  • the tube-shaped glass monolith fabricating method using a sol-gel process directs the gel to shrink from outside to inside during the drying step and unidirectionally dries the gel, thereby minimizing stresses of the gel caused by the gel shrinkage, and enabling a large crack-free glass tube for forming an optical fiber to be fabricated.
  • a high-purity optical fiber forming glass tube can be molded and product cost is reduced. This method can be applied to large, high-purity monolith fabrication.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacturing & Machinery (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Manufacture, Treatment Of Glass Fibers (AREA)
  • Glass Melting And Manufacturing (AREA)
US09/037,525 1997-03-10 1998-03-10 Apparatus and method for fabricating tube-shaped glass monolith using sol-gel process Expired - Fee Related US5922099A (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
KR1019970007976A KR100241969B1 (ko) 1997-03-10 1997-03-10 솔-젤법을이용한튜브형유리단일체제조장치
KR1019970007972A KR100229899B1 (ko) 1997-03-10 1997-03-10 솔-젤법을 이용한 튜브형 유리 단일체 제조방법
KR97-7972 1997-03-10
KR97-7976 1997-03-10

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JP (1) JP2891984B2 (ja)
CN (1) CN1188360C (ja)
DE (1) DE19810132C2 (ja)
FR (1) FR2760448B1 (ja)
GB (1) GB2323084B (ja)
RU (1) RU2144007C1 (ja)

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20010029756A1 (en) * 2000-04-18 2001-10-18 Samsung Electronic Co, Ltd. Apparatus and method for fabricating holey optical fiber
US6467312B1 (en) * 2000-07-11 2002-10-22 Fitel Usa Corp. Sol gel method of making an optical fiber with multiple apetures
US6546756B1 (en) * 1999-12-27 2003-04-15 Corning Incorporated Method of making an optical fiber, with storage in a new bag
US6555048B1 (en) * 1999-08-26 2003-04-29 Samsung Electronics Co., Ltd. Method for manufacturing tube-shaped silica glass product
US6598429B1 (en) 2000-11-17 2003-07-29 Beamtek, Inc. Method for fabricating gradient-index rods and rod arrays
US20030147605A1 (en) * 2002-02-01 2003-08-07 Shiho Wang Sol-gel-derived optical fiber preform and method of manufacture
US20030147606A1 (en) * 2002-02-01 2003-08-07 Shiho Wang Sol-gel-based optical preforms and methods of manufacture
US20030148053A1 (en) * 2002-02-01 2003-08-07 Shiho Wang Apparatus and method for forming a sol-gel monolith utilizing multiple casting
US20030151173A1 (en) * 2002-02-01 2003-08-14 Shiho Wang Method of removing liquid from pores of a sol-gel monolith
US20030174973A1 (en) * 2002-03-15 2003-09-18 Futoshi Ishii Connector component for optical fiber, manufacturing method thereof and optical member
US20040050113A1 (en) * 2001-10-18 2004-03-18 Soon-Cheol Hwang Preform for glass ferrule and fabrication method thereof
US20040050110A1 (en) * 2002-08-29 2004-03-18 Berkey George E. Methods for fabricating optical fibers and optical fiber preforms
US20040176758A1 (en) * 2003-03-04 2004-09-09 Cardiva Medical, Inc. Apparatus and methods for closing vascular penetrations
US20050072192A1 (en) * 2001-12-21 2005-04-07 Marco Arimondi Process for manufacturing a micro-structured optical fibre
US20050280180A1 (en) * 2002-05-14 2005-12-22 Chris Cunningham Method for making holder
WO2006047355A2 (en) * 2004-10-25 2006-05-04 Demodulation, Inc. Optically encoded glass-coated microwire
US20070095107A1 (en) * 2003-05-30 2007-05-03 Stefano Solinas Method and apparatus for forming a preform for a micro-structured optical fiber
US20080223786A1 (en) * 2007-03-13 2008-09-18 Varian, Inc. Methods and devices using a shrinkable support for porous monolithic materials
CN101298360B (zh) * 2008-06-04 2010-11-24 常熟市伟恒模具铸造有限公司 加工玻璃容器的模具
US10053386B2 (en) * 2014-04-25 2018-08-21 Corning Incorporated Method for forming optical fiber and preforms

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KR100617713B1 (ko) * 2004-02-12 2006-08-28 삼성전자주식회사 다공 광섬유의 제조방법

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Cited By (33)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6555048B1 (en) * 1999-08-26 2003-04-29 Samsung Electronics Co., Ltd. Method for manufacturing tube-shaped silica glass product
US6546756B1 (en) * 1999-12-27 2003-04-15 Corning Incorporated Method of making an optical fiber, with storage in a new bag
US6705126B2 (en) * 2000-04-18 2004-03-16 Samsung Electronics Co, Ltd. Method for fabricating holey optical fiber
US20010029756A1 (en) * 2000-04-18 2001-10-18 Samsung Electronic Co, Ltd. Apparatus and method for fabricating holey optical fiber
US6467312B1 (en) * 2000-07-11 2002-10-22 Fitel Usa Corp. Sol gel method of making an optical fiber with multiple apetures
US6598429B1 (en) 2000-11-17 2003-07-29 Beamtek, Inc. Method for fabricating gradient-index rods and rod arrays
US7467528B2 (en) * 2001-10-18 2008-12-23 Research Institute Of Industrial Science & Technology Method of fabricating dual hole glass ferrules
US20040050113A1 (en) * 2001-10-18 2004-03-18 Soon-Cheol Hwang Preform for glass ferrule and fabrication method thereof
US7779651B2 (en) 2001-12-21 2010-08-24 Prysmian Cavi E Sistemi Energia S.R.L. Process for manufacturing a micro-structured optical fibre
US20050072192A1 (en) * 2001-12-21 2005-04-07 Marco Arimondi Process for manufacturing a micro-structured optical fibre
US20030151173A1 (en) * 2002-02-01 2003-08-14 Shiho Wang Method of removing liquid from pores of a sol-gel monolith
US20030148053A1 (en) * 2002-02-01 2003-08-07 Shiho Wang Apparatus and method for forming a sol-gel monolith utilizing multiple casting
US6928220B2 (en) 2002-02-01 2005-08-09 Simax Technologies, Inc. Sol-gel-derived optical fiber preform and method of manufacture
US7000885B2 (en) 2002-02-01 2006-02-21 Simax Technologies, Inc. Apparatus and method for forming a sol-gel monolith utilizing multiple casting
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US20030147605A1 (en) * 2002-02-01 2003-08-07 Shiho Wang Sol-gel-derived optical fiber preform and method of manufacture
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DE19810132C2 (de) 2002-02-07
GB2323084A (en) 1998-09-16
JP2891984B2 (ja) 1999-05-17
JPH10251027A (ja) 1998-09-22
CN1201764A (zh) 1998-12-16
GB2323084B (en) 1999-05-12
CN1188360C (zh) 2005-02-09
FR2760448A1 (fr) 1998-09-11
DE19810132A1 (de) 1998-09-17
RU2144007C1 (ru) 2000-01-10
FR2760448B1 (fr) 1999-11-12

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